HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Iodine → 4-Iodo-1,2-dimethylbenzene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Iodine | HCID 807 | — |
| Edukt | O-Xylene | HCID 7237 | — |
| Katalysator | Silver(I) trifluoromethanesulfonate | HCID 76223 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 4-Iodo-1,2-dimethylbenzene | HCID 141646 | 78% |
Reaktionsschritte
A mixture of 1,2-dimethylbenzene (1.06 g; 10 mmol), silver trifluoromethanesulfonate (2.56 g; 10 mmol) and I2 (2.53 g; 10 mmol) in CH2Cl2 (50 ml) was stirred for 7 h at room temperature, then filtered through a Celite pad, washed with fresh CH2Cl2 (2×20 ml) and combined filtrates were washed with 5% Na2SO3, H2O, brine and dried over anhydrous MgSO4 and filtered. The filtrate was evaporated to dryness under reduced pressure to give crude title compound (1.8 g; 78%) as brownish oil, which was used in next step without further purification. 1H-NMR (CDCl3) 2.23 (s, 6H), 6.84 (d, 1H, J=8.0 Hz); 7.39 (dd, 1H, J=1.7; 8.0 Hz); 7.46 (broad s, 1H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09181182B2 |
| Quelldatensatz | uspto-grants-2015_11 |
| ORD ID | ord-e3f873ee157f4ab79c2246584636dcf2 |
| Quellennotiz | uspto-grants-2015_11 |